Apparatus for extracting nicotin.



Nor 678,39l. Patented luly l6, [90L H. FROEHLING.

APPARATUS FOR EXTRACTING NIGOTIN.

(Application filed Sept. 26 1900.) (lo llodol.)

3 M 1:01 1'01, Hen/y nae bah Witnesses THE mums PETKRS co. vno'mumo" wnsmnumu. n. cy

UNITED STATES PATENT OFFICE;

HENRY FROEHLING, OF RICHMOND, VIRGINIA, ASSIGNOR TO PASCAL DAVIE,

- OF SAME PLACE.

APPARATUS FOR EXTRACTING NICOTIN.

SPECIFIQATION forming part of Letters Patent No. 678,391, dated July 16, 1901.

Application filed september 28, 1900i Serial No. 31,422. (No model.)

T at whom it may concern:

Be it known that I, HENRY FROEHLING, a citizen of the United States, residing at Richmond, in the county of Henrico and State of Virginia, have invented certain new and useful Improvements in Apparatus for Extracting Nicotin and Oil from Tobacco, &c'.; and I do hereby declare the following to be a full, clear, and exact description of the invention,

to such as will enable others skilled inthe art to which it appertains to make and use the same.

My invention relates to improvements in apparatus for extracting nicotin and oils from r 5 tobacco and tobacco-stems or other alkaloids and oils from stems, barks, leaves, seeds, and the like.

It consists in ;an apparatus comprising a receptacle for holding the materials to be opzo erated upon and for receiving the extracting agents to be applied thereto, a still for receivingthe extracting agent laden with alkaloids and oils and for separating and driving off the said extracting agent by volatilizat-i'on,

2 5 meansfor leading the said extracting agent back into the said receptacle while it is in a volatilized condition, and means for applying a cooling agent to the said receptacle for condensing the said agent therein and while in contact with the mate-rials within the receptacle.

It further consists in an apparatus for treating tobacco comprising a receptacle for inclosinga suitable quantity of it, the said receptacle being supplied with a charge of hydrocarbon or other extracting agent for acting upon the tobacco, a trap for receiving the agent laden with the substances extracted and arranged so as to separate water and 40 alkaloids with which the tobacco was prepared for treatment from the extracting agent, nicotin, and oils, a still connected with the trap, so as to receive the said agent, alkaloids, and

tilized agent into the receptacle again in which it is condensed while acting on its contents.

It also consists of certain other novel constructions, combinations, and arrangements of parts, as will be hereinafter fully described I and claimed.

In the accompanying drawing the figure represents a side elevation of an apparatus embodying the features of this invention.

The drawing illustrates a practical embodiment of the invention, in which is shown a cylindrical receptacle 1 for containing charges of tobacco for treatment. A hydrocarbon or other extracting agent is indroduced from time to time into the receptacle 1 from a supply-tank 5 through a pipe 22, controlled by a cook 24. A water trap 4 receives the liquids draining from the receptacle 1 and separates therefrom the water and alkaloids which they contain. The extracting agent with the nicotin passes into a still 2, wherein the said agent is volatilized and driven off to return to the receptacle 1 in the form .of vapor. The vapor is condensed again in the said receptacle, acting upon the contents thereof both in its volatilized and condensed condition. To facilitate the condensing of the extracting agent in the receptacle, the said receptacle is formed with double Walls constituting a jacket 6, which may be supplied through a pipe 7 with any suitable cooling agent, as water or a cooling-brine. The jacket 6 is provided with draw-0E cocks, as 8 and 9, through which the contents of the jacket may be removed, or a continuous flow of substance may be maintained through the said jacket, if desired.

The cylinder 1 is provided with a removable top 10 and a removable bottom 11, similar in construction to the top and adapted to be held in place by an-inclosing frame 12,

which has cross pieces or bars 13 and 14 at the top and bottom. Clamping-screws 15 and 16 are carried by the said crossbars 13 and 0 14 and engage sunken portions at the centers of the said top and bottom 10 and 11; By securing the set-screws 15 and 16 tightly against oils, means for heating the still for separating 45 and driving off the extracting agent by volatilization, and means for delivering the vola-" the said covers theycan be snugly held in position. The bottom 11 carries an inner false 9 bottom 17, which is perforated, so that liquid in the receptacle 1 may trickle through the said bottom and be carried off by a pipe 18, provided for that purpose, which enters through the bottom 11 and leads to the wa- ICG tor-trap 4. The flow of substances through the pipe 18 is controlled by a valve or cook 19. A pipe 20 also passes out from the bottom 11 to afford another exit for the contents of the receptacle when required. -A draw-off cock, as 44, is alsoapplied to the bottom of the receptacle 1, through which some of its contents may be removed from time to time to ascertain the condition thereof.

Thepipe 18 passes into the trap 4 and to a point near the bottom thereof. leads from the trap 4 at a point near its upper end to the still 2 and is controlled by a cook 26. The trap is also provided with a draw-oil cock 57, arranged on a level lower than the outlet 25, throughwhich water and alkalies collected in the trap may be drawn oif from time to time, so that the same will never enter the still with the nicotin and extracting agent. The trap also has a drawolt cock 56 at its lower end.

The still 2 is supported in any suitable man-- ner and is preferably formed with an upper section 27 and a lower section 28, provided with meeting fianges,which may be bolted or riveted together, as illustrated in the drawings. The still has a gage 29 and a thermometer 30, so that the condition of the contents of the said still may be readily ascer .tained at a glance.- Both the pipe '7 and the pipe 32, leading from the still-jacket, are connected by a suitable coupling with a heatingpipe 33 and also a cooling-pipe 34 by means of a connecting-pipe 35. Valves 36, 37, and 38 control this piping. The lower part 28 of the still is provided with a jacket 31, connected, as above intimated, with the pipe 32, so that steam or other heating agents may be brought into the said jacket for heating the still, and so, also, a cooling agent may be used in the still-jacket when required. The still 2 is further provided with a drain-pipe 41, which enters at the bottom of the still and is controlled by a valve 42. A draw-oif cock 43 is also arranged upon the bottom of the still, so that samples of its contents may be removed at any time for examination. The still is connected with the receptacle 1 by means of piping 45 and 47, controlled by cocks 48 and 50, so that the extracting agent used in this apparatus when Volatilized in the still may be led therefrom in this condition to the said receptacle 1. The tank 5 for supplying the liquid-extracting agent to the apparatus is a closed receptacle provided with a suitable air-vent. The tank is also provided with an inlet-pipe 55, by which airpressure may be supplied thereto for forcing its contents into the receptacle 1 through the pipe 22. A valve or cook 2t controls the said pipe 22.

The condenser 3 is conveniently arranged with respect to the receptacle 1 and the still 2 and comprises a receptacle or casing connected by a pipe 39 with the cold supply-pipe 34, so that a cooling agent maybe introduced A pipe oraeei into said casing, a valve 40 in the pipe 39 regulating such introduction. An overflowpipe 54 is used to maintain the proper height of the cooling substance in the condenser. A coil of pipe 46 is located in the condenser and leads from the piping and -through the condenser to the pipe 52, by which it is connected to the supply-tank 5, and is provided with a valve 53. A branch pipe 21, provided with a valve 23, connects the coil 46 with the receptacle 1, so that it may act as a refluxcondenser for said receptacle. The coil 46 may be shut oil? from the piping 45 and 47 by a cock 49. A safety-valve 51 is located at the juncture of the coil with the said piping 45 and 47.

In using this apparatus for the extraction of nicotin from tobacco, for which purpose the apparatus is primarily designed, the receptacle lis filled, say, to within twoor three inches of the top with granulated tobacco or comminuted tobacco-stems. preferably moistened, as is usualwhen nicotin is to be extractedtherefrom, by a hydrocarbon extracting agent with lime water, caustic soda, or some other alkaline solution, which, as is well known, aifects the same so that the nicotin will be readily attacked by the hydrocarbon or other extracting agent used. A charge of gasolene or other hydrocarbon extracting agent is then admitted to the receptacle 1 from the supply-tank 5, after which the valve 24 may be closed until another charge of material is desired. The extracting agent will percolate through the tobacco, carrying nicotin and other oils with it, and will pass out the pipe 18 to the trap 4. In this trap the moisture and alkali with which the tobacco was previously prepared and which has come with the nicotin and extracting agent from the receptacle 1 will be completely separated from the said nicotin and extracting agent, the said alkali and water sinking to the bottom of the trap, while the lighter hydrocarbon, nicotin, and other oils will rise to the top and pass through the pipe 25 into the still 2. In the still the substances received from the water-trap are subjected to sufiicient heat to drive oil the extracting agent in the form of a vapor. The said extracting agent may then in its volatilized condition be led through the piping 45 and 47 to the receptacle 1 again, the valves 48 and 50 having been opened for this purpose. By this means the upper part of the charge of tobacco in the receptacle, which will not be submerged in the liquid extracting agent standing in the lower portion of the said receptacle, will be thoroughly permeated by the volatilized extracting agent. After reaching .the receptacle 1 again the volatilized agent will be gradually condensed, settling to the bottom of the receptacle in its liquid form, and can be made to pass around through the apparatus again, as just described, until the charge of tobacco ,has been sufficiently de- The tobacco is prived of its nicotin. In order to facilitate the condensing of the volatilized agent in the receptacle 1 and greatly hasten the operation, 1 preferably introduce a cooling agent through the pipes 34, 35, and 7 into the jacket 6, using a cooling-brine or merely cooling-water, as may be preferred. The condenser 3 may also be used as a reflux-condenser for assisting in the condensing operation by opening the valve 23 in the pipe 21 and closing the valve 46. In this way whatever vaporized extracting'agent may rise'through the pipe 21 into the coil 46 of the condenser will be condensed therein and will run back into the receptacle 1. When the operation has been carried far enough, the extracting agent instead of being returned from the still to the receptacle 1 will be passed through the condenser 3, the cook 46 being opened for this purpose and the cock 50 being closed. By closing the cock 28 and opening the cock 53 the extracting agent as it becomes condensed will run from the coil 46 through the pipe 52 back to the supply-tank 5. After all of the extracting agent has been returned to the tank 5 that can be recovered in this manner some fumes of the samewill probably remainwith the tobacco in the receptacle 1.

' To drive these olf, the condenser is connected with the receptacle 1 again by opening the valve 23, the valve 46 having been closed, when by removing the cooling agent from the jacket 6 and introducingsteam thereto from the pipe 33 through the pipe 7 the remaining traces of hydrocarbon may be volatilized and driven up into the condenser, where it will again be liquefied and permitted to pass through the pipe 52 into the tank 5. The nicotin and oils collected in the still may be permitted to cool as they-stand in the said still; but the cooling operation is preferably hastened by shutting off" the steam from the still-jacket and introducing the cooling agent therein. It is of course necessary to 'cool the nicotin before it can be removed from the still and handled where any one can breathe the atmosphere, since it is dangerous to breathe the fumes of the violent poison nicotin which would arise from the same when in a heated condition. After the exhausted tobacco has been removed from the receptacle 1 a new charge can be inserted therein and the extracting agent applied to, the same, as before, for repeating the operation.

The use of the trap 4 con tributes largely to the successful handling of the nicotin in this apparatus, for it is well known that when nicotin is subjectedto heat in the presence of an alkali the nicotin will be decomposed and driven off. If, therefore, the alkali and water were permitted to pass into the still 2 and therein subjected to heat when the extracting agent was being volatilized, the nicotin would be decomposed and driven off with the said extracting agent, thereby largely frustrating the attempt to collect the nicotin. The nicotin in this case would of course pass back intothe receptacle 1 with the volatilized extracting agent and practically nothing would be gained by the operation. The use of the trap 4, however, entirely removes the water and alkalies from the liquids passing to the still, and the said water and alkalies may be drawn olf from the trap from time to time before a sufficient quantity has collected toreach the outlet from the said trap to the still. The upper draw-01f cock 57 of the said trap is arranged, as will be seen in the drawings, upona level lower than the outlet-pipe 25, which communicated with the still.

Theapparatus above described, while designed especially for the extraction of nicotin from tobacco and while being adapted for accomplishing that purpose in a very perfoot manner, is capable also of use in extracting oils from "various materials, which may be placed in the receptacle 1 and treated with an extracting agent. In processes of this character it is usually not needful to apply a cooling agent to the extracting-receptacle; but means for accomplishing this purpose does form an important feature in the extraction of nicotin from tobacco.

Having thus described my invention, What I claim as new, and desire to secure by Letters Patent, is-

1. An apparatus for extracting oil, nicotin or alkaloids from vegetable substances, comprising a cylinder, a still connected therewith,

and a supply-tank adapted to introduce extracting agents in a liquid state into the top of the cylinder, means for leading the Volatilized agents fromthe still to the said cylinder, and means for continuously condensing the volatilized agents after they enter the cylinder and while in contact with the material in the cylinder, the structure being such that r a continuous circulation of gases or fluids may be effected through the said cylinder, substantially as described.

2. An apparatus for extracting oil, nicotin and alkaloids from vegetable materials, comprising a cylinder, removable covers for closing the ends of said'cylinder, a closed water-trap for receiving the liquids from the cylinder, astill connectedwith the water-trap for receiving the gases or oils from said watertrap, and means for applying a low temperature to the walls of the cylinder for continuously condensing the entering volatilized agent after it has been in contact with the contents of the cylinder a while and so that it will engage the said contents in a liquid state before passing from the cylinder, and means for applying heat afterward to the walls of the cylinder to drive off all of the volatile extracting agent before removing the residuum, and similar means for heating or cooling the'said still as may be desired, sub

stantially as described.

oil from tobacco or similar substances, comprising an extracting-receptacle, a still 'connected with the said receptacle so as to receive substances passing therefrom, a pipe leading from the said still to the extractingcylinder through which the volatilized extracting agent may flow, a cooling-jacket applied to the extracting-receptacle and a supply-tank for delivering quantities of the extracting agent to the extracting-cylinder as the case may require, substantially as described.

4. In an apparatus for extracting nicotin and oil from tobacco and other substances, the combination of an extractirig-receptacle, a still connected with the said receptacle so as to receive liquids therefrom, a trap interposed between the still and the receptacle for separating water and alkaline substances from said liquid, a pipe leading from the still to the extracting-cylinder through which the volatilized extracting agent may flow, and means for condensing the volatilized agent in the said receptacle, substantially as described.

5. An apparatus for extracting nicotin and alkaloids from'tobacco or other similar substances, comprising an extracting-receptacle, a still for receiving the alkaloids and associated products from the said receptacle, a trap interposed between the receptacle and still for preventing the passage of any alkaline liquids with the said products into the said still, a pipe for leading the extracting agent in a volatilized form back to the extracting-receptacle,means forapplyinga cooling agent to the receptacle for condensing the volatilized extracting agent therein, a condenser also connected with the receptacle for assisting in the condensing operation, any vapor which may pass to the same from the receptacle being condensed therein and returned to the receptacle in a liquid form and a supply-tank for furnishing the extractingreceptacle with the extracting agent as occasion may require, substantially as described.

6. An apparatus for extracting nicotin or alkaloids from tobacco or other similar substances, comprising an extracting-receptacle, a still for receiving liquids passing from the said receptacle, a trap interposed between the still and receptacle for removing water and alkaline substances from the said liquids, a pipe for returning the extracting agent from the still to the receptacle in a volatilized condition, means for applying a cooling agent to the receptacle for facilitating the condensing of the vaporized agent which has been returned to the extracting-receptacle, a supplytank for delivering the required extracting agent to the receptacle, a condenser through which the extracting agent may be passed from the still and reduced to a liquefied condition on its way back to the supply-tank when the charge of material in the receptacle has been relieved of all of its nicotin, and means for heating the exhausted contents of the receptacle for driving olf any remaining fumes of the extracting agent into the condenser before the receptacle is emptied and prepared for a new charge, substantially as described.

7. An apparatus for extracting nicotin from tobacco, comprising a receptacle for receiving a charge of the tobacco to be treated, a supply-tank for delivering an extracting agent to the receptacle as may be needed, a pipe leading from the receptacle to the bottom of a water-trap, a Water-trap surrounding the end of said pipe for receiving liquids which drain from the receptacle, an outletpipe leading from the upper part of the tank to a still, whereby the nicotin and lighter oils will be permitted to flow into the still, while water and alkaline materials with which the tobacco was prepared for the operation, will be detained in the tank, means for drawing the water and alkaline substances from the tank at a level lower than the outlet to the still, a still for receiving the nicotin and associated products, a pipe for returning thev extracting agent in a volatilized condition from the still to the receptacle, means for heating the still for producing this volatilized condition of the extracting agent, and a cooling-jacket surrounding the extracting-receptacle for facilitating the condensation of the extracting agent after it has been returned to said receptacle, substantially as described.

8. An apparatus for extracting nicotin from tobacco or liquids from vegetable substances, comprising a cylinderhaving double walls forming a jacket around the same, covers for closing the ends of the cylinder, means for holding the said covers in position comprising a frame or yoke surrounding the cylinder,adjusting-screws mounted in said frame and engaging the covers, whereby they may be clamped to the ends of the cylinder, a still connected to the cylinder, and a supply-tank for holding extracting agents, and means for delivering the extracting agents to the cylinder in a liquid state, and means for passing the extracting agents from the still into the cylinder in a volatilized condition, and means for applying a cooling and a heating agent to the contents of the cylinder byintroducing the same into the jacket surrounding the cylinder, substantially as described.

9. An apparatus for extracting nicotin from tobacco or alkaloids from vegetable materials, comprising a receptacle for receiving the material, means for applying a cooling and a heating agent to the walls of the receptacle externally thereof, a Water-trap connected with the receptacle, a pipe leading from the receptacle into the water-trap and extending to a point in close proximity to the bottom of the trap, whereby the liquids passing from the receptacle will be introduced into the water-trap at a point considerably below its outlet, a pipe leading from the water-trap at a point near its upper end to a suitable still, a still for receiving oils and extracting agents from the Water-trap, receptacle from the still in avolatilized conthe said still comprising upper and lower dition, substantially as described. 10 shells or casings secured together at their In testimony whereof I hereunto affix my meeting edges, a jacket surrounding the signature in presence of two Witnesses.

lower shell for receiving heating or cool- HENRY FROEHLING. ing agents, means for delivering extracting Witnesses: agents to the receptacle in aliquid state, and PASCAL DAVIE,

means for delivering extracting agents to the E. T. FENWIOK. 

